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NASA NTRS1993

Studies of the net surface radiative flux from satellite radiances during FIFE

Studies of the net surface radiative flux from satellite radiances during First ISLSCP Field Experiment (FIFE) are presented. Topics covered include: radiative transfer model validation; calibration of VISSR and AVHRR solar channels; development and refinement of algorithms to estimate downward solar and terrestrial irradiances at the surface, including photosynthetically available radiation (PAR) and surface albedo; verification of these algorithms using in situ measurements; production of maps of shortwave irradiance, surface albedo, and related products; analysis of the temporal variability of shortwave irradiance over the FIFE site; development of a spectroscopy technique to estimate atmospheric total water vapor amount; and study of optimum linear combinations of visible and near-infrared reflectances for estimating the fraction of PAR absorbed by plants.

Frouin, Robert↗

NASA NTRS2002

Chemical Detection and Identification Techniques for Exobiology Flight Experiments

Exobiology flight experiments require highly sensitive instrumentation for in situ analysis of the volatile chemical species that occur in the atmospheres and surfaces of various bodies within the solar system. The complex mixtures encountered place a heavy burden on the analytical Instrumentation to detect and identify all species present. The minimal resources available onboard for such missions mandate that the instruments provide maximum analytical capabilities with minimal requirements of volume, weight and consumables. Advances in technology may be achieved by increasing the amount of information acquired by a given technique with greater analytical capabilities and miniaturization of proven terrestrial technology. We describe here methods to develop analytical instruments for the detection and identification of a wide range of chemical species using Gas Chromatography. These efforts to expand the analytical capabilities of GC technology are focused on the development of detectors for the GC which provide sample identification independent of the GC retention time data. A novel new approach employs Penning Ionization Electron Spectroscopy (PIES).

Kojiro, Daniel R.↗

NASA NTRS2002

Analytical/Operational Requirements for the In Situ Chemical Analysis of Cometary and Planetary Environments Using GC-IMS

Exobiology flight experiments require highly sensitive instrumentation for the in situ analysis of the volatile chemical species that occur in the atmospheres and surfaces of various bodies within the solar system. The complex mixtures encountered place a heavy burden on the analytical instrumentation to detect and identify all species present. The minimal resources available onboard for such missions mandate that the instruments provide maximum analytical capabilities with minimal requirements of volume, weight and consumables. The miniCIDEX instrument was developed for the chemical analysis of a cemetery environment. It combined a Gas Chromatograph (GC) with a helium based Ion Mobility Spectrometer (IMS) to fulfill the analytical requirements of a cemetery exobiology mission: universal response; ppb sensitivity; low mass, volume and consumable MiniCIDEX is now a candidate for the chemical analysis instrument of a Titan Aero-rover Mission. The complexity of the analyses will be similar to the comet application with a heavier emphasis on organic molecules. Because the Titan Aero-Rover will be a balloon powered rover, much more attention is placed on the total mass of the instrument package. The GC will likely be a Micro-Electro-Mechanical-System (MEMS) design, smaller than the initial miniCIDEX GC by a factor of ten (with a similar reduction in consumable use). Similar miniaturization of the helium-based IMS will be necessary while maintaining the analytical capabilities. The two mission applications, the analytical requirements, and the evolution of the IMS design to accommodate these requirements will be presented.

Kojiro, Daniel R.↗

NASA NTRS2006

Miniature GC: Minicell ion mobility spectrometer (IMS) for astrobiology planetary missions

Kojiro, Daniel R.↗

NASA NTRS2006

Miniature GC-Minicell Ion Mobility Spectrometer (IMS) for In Situ Measurements in Astrobiology Planetary Missions

Astrobiology flight experiments require highly sensitive instrumentation for in situ analysis of volatile chemical species and minerals present in the atmospheres and surfaces of planets, moons, and asteroids. The complex mixtures encountered place a heavy burden on the analytical instrumentation to detect and identify all species present. The use of land rovers and balloon aero-rovers place additional emphasis on miniaturization of the analytical instrumentation. In addition, smaller instruments, using tiny amounts of consumables, allow the use of more instrumentation and/or ionger mission life for stationary landers/laboratories. The miniCometary Ice and Dust Experiment (miniCIDEX), which combined Gas Chromatography (GC) with helium Ion Mobility Spectrometry (IMS), was capable of providing the wide range of analytical information required for Astrobiology missions. The IMS used here was based on the PCP model 111 IMS. A similar system, the Titan Ice and Dust Experiment (TIDE), was proposed as part of the Titan Orbiter Aerorover Mission (TOAM). Newer GC systems employing Micro Electro- Mechanical System (MEMS) based technology have greatly reduced both the size and resource requirements for space GCs. These smaller GCs, as well as the continuing miniaturization of Astrobiology analytical instruments in general, has highlighted the need for smaller, dry helium IMS systems. We describe here the development of a miniature, MEMS GC-IMS system (MEMS GC developed by Thorleaf Research Inc.), employing the MiniCell Ion Mobility Spectrometer (IMS), from Ion Applications Inc., developed through NASA's Astrobiology Science and Technology Instrument Development (ASTID) Program and NASA s Small Business Innovative Research (SBIR) Program.

Kojiro, Daniel R.↗

DOE OSTI2020

Identifying and Tuning the In Situ Oxygen-Rich Surface of Molybdenum Nitride Electrocatalysts for Oxygen Reduction

Rigorous in situ studies of electrocatalysts are required to enable the design of higher performing materials. Nonplatinum group metals for oxygen reduction reaction (ORR) catalysis containing light elements such as O, N, and C are known to be susceptible to both ex situ and in situ oxidation, leading to challenges associated with ex situ characterization methods. We have previously shown that the bulk O content plays an important role in the activity and selectivity of Mo–N catalysts, but further understanding of the role of composition and morphological changes at the surface is needed. Here, we report the measurement of in situ surface changes to a molybdenum nitride (MoN) thin film under ORR conditions using grazing incidence X-ray absorption and reflectivity. We show that the half-wave potential of MoN can be improved by ~90 mV by potential conditioning up to 0.8 V versus RHE. Utilizing electrochemical analysis, dissolution monitoring, and surface-sensitive X-ray techniques, we show that under moderate polarization (0.3–0.7 V vs RHE) there is local ligand distortion, O incorporation, and amorphization of the MoN surface, without changes in roughness. Furthermore, with a controlled potential hold procedure, we show that the surface changes concurrent with potential conditioning are stable under ORR relevant potentials. Conversely, at higher potentials (≥0.8 V vs RHE), the film incorporates O, dissolves, and roughens, suggesting that in this higher potential regime, the performance enhancements are due to increased access to active sites. Density functional theory calculations and Pourbaix analysis provide insights into film stability and O incorporation as a function of potential. These findings coupled with in situ electrochemical surface-sensitive X-ray techniques demonstrate an approach to studying nontraditional surfaces in which we can leverage our understanding of surface dynamics to improve performance with the rational, in situ tuning of active sites.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS2012

NASA Tech Briefs, November 2012

The topics include: Visual System for Browsing, Analysis, and Retrieval of Data (ViSBARD); Time-Domain Terahertz Computed Axial Tomography NDE System; Adaptive Sampling of Time Series During Remote Exploration; A Tracking Sun Photometer Without Moving Parts; Surface Temperature Data Analysis; Modular, Autonomous Command and Data Handling Software with Built-In Simulation and Test; In-Situ Wire Damage Detection System; Amplifier Module for 260-GHz Band Using Quartz Waveguide Transitions; Wideband Agile Digital Microwave Radiometer; Buckyball Nucleation of HiPco Tubes; FACT, Mega-ROSA, SOLAROSA; An Integrated, Layered-Spinel Composite Cathode for Energy Storage Applications; Engineered Multifunctional Surfaces for Fluid Handling; Polyolefin-Based Aerogels; Adjusting Permittivity by Blending Varying Ratios of SWNTs; Gravity-Assist Mechanical Simulator for Outreach; Concept for Hydrogen-Impregnated Nanofiber/Photovoltaic Cargo Stowage System; DROP: Durable Reconnaissance and Observation Platform; Developing Physiologic Models for Emergency Medical Procedures Under Microgravity; Spectroscopic Chemical Analysis Methods and Apparatus; Low Average Sidelobe Slot Array Antennas for Radiometer Applications; Motion-Corrected 3D Sonic Anemometer for Tethersondes and Other Moving Platforms; Water Treatment Systems for Long Spaceflights; Microchip Non-Aqueous Capillary Electrophoresis (MicronNACE) Method to Analyze Long-Chain Primary Amines; Low-Cost Phased Array Antenna for Sounding Rockets, Missiles, and Expendable Launch Vehicles; Mars Science Laboratory Engineering Cameras; Seismic Imager Space Telescope; Estimating Sea Surface Salinity and Wind Using Combined Passive and Active L-Band Microwave Observations; A Posteriori Study of a DNS Database Describing Super critical Binary-Species Mixing; Scalable SCPPM Decoder; QuakeSim 2.0; HURON (HUman and Robotic Optimization Network) Multi-Agent Temporal Activity Planner/Scheduler; MPST Software: MoonKommand

Source record↗

NASA NTRS2008

Miniature Mass Spectrometers on Space and Planetary Missions

Space flight mass spectrometers contribute our understanding of the origin and evolution of our solar system and even of life itself. This fundamental role has motivated increasing interest in miniature mass spectrometry for planetary missions. Several remarkable new instruments are en route or under development to investigate the composition of planetary bodies such as Mars and comets. For instance, the Sample Analysis at Mars (SAM) suite on the 2009 Mars Science Laboratory (MSL) mission includes a quadrupole mass spectrometer with a sophisticated gas processing system as well as pyrolysis and chemical derivatization protocols for solid samples. Future missions will require even lighter, lower power, and yet more capable mass spectrometers, particularly to analyze samples in situ on planetary surfaces. We have been developing laser-based mass spectrometers for elemental and organic/molecular analysis of rock, ice, or fine particle samples. These typically use time-of-flight (TOF) mass analyzers, which are readily miniaturized and can detect both atomic species and complex organics that occur in a variety of planetary materials. For example, nonvolatile polycyclic aromatic hydrocarbons and kerogen-like macromolecular carbon are found in some carbonaceous meteorites, which derived from asteroid parent bodies. A single focused laser pulse is able to volatilize and ionize some of these compounds for direct TOF analysis. While this is possible without any sample preparation or contact, sensitivity and quantitative performance can improve significantly with some sample handling. As such we have also been examining robotic mechanisms and protocols to accompany space flight mass spectrometers. In addition, sensors in early development may significantly improve these capabilities, via use of techniques such as switchable polarity, ambient pressure, or resonant ionization; tandem mass spectrometry (TOF or ion trap); and chemical imaging.

Brinckerhoff, William↗

DOE OSTI2026

Impacts of A‐Site Composition on the Cation Dissolution‐Mediated Surface Restructuring of Layered Nickelate Oxide Electrocatalysts During Alkaline Oxygen Evolution Reaction

The oxygen evolution reaction (OER) is a key anodic counter‐reaction for electrochemical production of fuels and chemicals. It is hindered by sluggish four‐electron transfer kinetics requiring highly oxidative operating potentials to achieve commercially relevant rates. NiFeO x H y electrocatalysts are among the most promising for OER in alkaline electrolytes. The Ni(OH) 2 /NiOOH redox couple has been reported as the active phase in Ni‐based electrocatalysts; however, its activity is often hindered by deactivation arising from the formation of OER‐inactive insulating species. Limited strategies exist for mitigating this deactivation. This study aims to address this by interrogating the evolution of OER active sites as a function of precatalyst composition and structural properties using a series of layered, crystalline Ni‐based Ruddlesden–Popper (RP) oxides (A 2 NiO 4+δ ). In situ evolution of the active NiO x H y surface is probed through Ni‐site OER turnover frequency analysis, and electrochemical impedance spectroscopy coupled with scanning transmission electron microscopy. We show that the stability of layered nickelate oxide electrocatalysts is governed by the dynamic competition between cation dissolution and Ni‐site reversibility, which can be tuned through the A‐site composition of RP oxides. These findings yield insights toward engineering OER oxide precatalysts that optimize the stability of in situ‐generated OER active phases.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2023

Machine-learning-assisted analysis of transition metal dichalcogenide thin-film growth

In situ reflective high-energy electron diffraction (RHEED) is widely used to monitor the surface crystalline state during thin-film growth by molecular beam epitaxy (MBE) and pulsed laser deposition. With the recent development of machine learning (ML), ML-assisted analysis of RHEED videos aids in interpreting the complete RHEED data of oxide thin films. The quantitative analysis of RHEED data allows us to characterize and categorize the growth modes step by step, and extract hidden knowledge of the epitaxial film growth process. In this study, we employed the ML-assisted RHEED analysis method to investigate the growth of 2D thin films of transition metal dichalcogenides (ReSe2) on graphene substrates by MBE. Principal component analysis (PCA) and K-means clustering were used to separate statistically important patterns and visualize the trend of pattern evolution without any notable loss of information. Using the modified PCA, we could monitor the diffraction intensity of solely the ReSe2 layers by filtering out the substrate contribution. These findings demonstrate that ML analysis can be successfully employed to examine and understand the film-growth dynamics of 2D materials. Further, the ML-based method can pave the way for the development of advanced real-time monitoring and autonomous material synthesis techniques.

36 MATERIALS SCIENCE↗

NASA NTRS2021

Assimilation of SMAP Brightness Temperature Observations in the GEOS Land–Atmosphere Data Assimilation System

Errors in soil moisture adversely impact the modeling of land–atmosphere water and energy fluxes and, consequently, near-surface atmospheric conditions in atmospheric data assimilation systems (ADAS). To mitigate such errors, a land surface analysis is included in many such systems, although not yet in the currently operational NASA Goddard Earth Observing System (GEOS) ADAS. This article investigates the assimilation of L-band brightness temperature (Tb) observations from the Soil Moisture Active Passive (SMAP) mission in the GEOS weakly coupled land–atmosphere data assimilation system (LADAS) during boreal summer 2017. The SMAP Tb analysis improves the correlation of LADAS surface and root-zone soil moisture versus in situ measurements by ∼0.1–0.26 over that of ADAS estimates; the unbiased root-mean-square error of LADAS soil moisture is reduced by 0.002–0.008 m^3 /m^3 from that of ADAS. Furthermore, the global land average RMSE versus in situ measurements of screen-level air specific humidity (q2m) and daily maximum temperature (T2m_max ) is reduced by 0.05 g/kg and 0.04 K, respectively, for LADAS compared to ADAS estimates. Regionally, the RMSE of LADAS q2m and T2m_max is improved by up to 0.4 g/kg and 0.3 K, respectively. Improvement in LADAS specific humidity extends into the lower troposphere (below ∼700 mb), with relative improvements in bias of 15–25%, although LADAS air temperature bias slightly increases relative to that of ADAS. Finally, the root mean square of the LADAS Tb observation-minus-forecast residuals is smaller by up to ∼0.1 K than in a land-only assimilation system, corroborating the positive impact of the Tb analysis on the modeled land–atmosphere coupling.

microwave remote sensing↗

DOE OSTI2022

Emerging Electrochemical Techniques for Probing Site Behavior in Single-Atom Electrocatalysts

Single-atom catalysts (SACs) have aroused tremendous interest over the past decade, particularly in the community of energy and environment-related electrocatalysis. A rapidly growing number of recent publications have recognized it as a promising candidate with maximum atomic utilization, distinct activity, and selectivity in comparison to bulk catalysts and nanocatalysts. However, the complexity of localized coordination environments and the dispersion of isolated sites lead to significant difficulties when it comes to gaining insight into the intrinsic behavior of electrocatalytic reactions. Furthermore, the low metal loadings of most SACs make conventional ensemble measurements less likely to be accurate on the subnanoscale. Thus, it remains challenging to probe the activity and properties of individual atomic sites by available commercial instruments and analytical methods. In spite of this, continuing efforts have lately focused on the development of advanced measurement methodologies, which are very useful to the fundamental understanding of SACs. There have recently been a number of in situ/operando techniques applied to SACs, such as electron microscopy, spectroscopy, and other analysis methods, which support relevant functions to identify the active sites and reaction intermediates and to investigate the dynamic behavior of localized structures of the catalytic sites. This Account aims to present recent electrochemical probing techniques which can be used to identify single-atomic catalytic sites within solid supports. First, we describe the basic principles of molecular probe methods for the study and analysis of electrocatalytic site behavior. In particular, the in situ probing technique enabled by surface interrogation scanning electrochemical microscopy (SISECM) can measure the active site density and kinetic rate with high resolution. An alternative electrochemical probing technique is further demonstrated on the basis of single-entity electrochemistry, which allows the unique electrochemical imaging of the size and catalytic rate of single atoms, molecules, and clusters. Next, the merits and limitations of different electrochemical techniques are then discussed, along with perspectives for future prospects. Apart from this, we further showcase the powerful capability of emerging electrochemical probing techniques for determining significant effects and properties of SACs for various electrocatalytic reactions, including oxygen reduction and evolution, hydrogen evolution, and nitrate reduction. Overall, electrochemical techniques with atomic resolution have greatly increased opportunities for observing, measuring, and understanding the surface and interface chemistry during energy conversion. In the future, it is anticipated that the development of electrochemical probing techniques will be advanced with innovative perspectives on the behavior and features of SACs. We hope that this Account can contribute in several ways to promoting the fundamental knowledge and technical progress of emerging electrochemical measurements for studying SACs.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Characterization of plasma catalytic decomposition of methane: role of atomic O and reaction mechanism

In this work, we investigated atmospheric pressure plasma jet (APPJ)-assisted methane oxidation over a Ni-SiO 2 /Al 2 O 3 catalyst. We evaluated possible reaction mechanisms by analyzing the correlation of gas phase, surface and plasma-produced species. Plasma feed gas compositions, plasma powers, and catalyst temperatures were varied to expand the experimental parameters. Real-time Fourier-transform infrared spectroscopy was applied to quantify gas phase species from the reactions. The reactive incident fluxes generated by plasma were measured by molecular beam mass spectroscopy using an identical APPJ operating at the same conditions. A strong correlation of the quantified fluxes of plasma-produced atomic oxygen with that of CH 4 consumption, and CO and CO 2 formation implies that O atoms play an essential role in CH 4 oxidation for the investigated conditions. With the integration of APPJ, the apparent activation energy was lowered and a synergistic effect of 30% was observed. We also performed in-situ diffuse reflectance infrared Fourier-transform spectroscopy to analyze the catalyst surface. The surface analysis showed that surface CO abundance mirrored the surface coverage of CH n at 25 °C. This suggests that CH n adsorbed on the catalyst surface as an intermediate species that was subsequently transformed into surface CO. We observed very little surface CH n absorbance at 500 °C, while a ten-fold increase of surface CO and stronger CO 2 absorption were seen. This indicates that for a nickel catalyst at 500 °C, the dissociation of CH 4 to CHn may be the rate-determining step in the plasma-assisted CH 4 oxidation for our conditions. We also found the CO vibrational frequency changes from 2143 cm –1 for gas phase CO to 2196 cm –1 for CO on a 25 °C catalyst surface, whereas the frequency of CO on a 500 °C catalyst was 2188 cm –1 . Here, the change in CO vibrational frequency may be related to the oxidation of the catalyst.

methane oxidation↗

NASA NTRS1981

A study of model parameters associated with the urban climate using HCMM data

The use of infrared and visible data from the Heat Capacity Mapping Mission (HCMM) and in situ data to study the intensity of the urban heat island of Saint Louis is described. Analysis of HCMM data shows that an urban heat island exists day and night in all seasons when clear skies prevail. The lower albedo value of the urban region during the day suggests that the higher temperatures are due to more absorption of solar radiation. Preliminary analysis of in situ meteorological data was performed after merging with HCMM data, and surface roughness, the exchange coefficient, and the soil moisture were calculated.

Source record↗

NASA NTRS1990

International cooperation for Mars exploration and sample return

The National Research Council's Space Studies Board has previously recommended that the next major phase of Mars exploration for the United States involve detailed in situ investigations of the surface of Mars and the return to earth for laboratory analysis of selected Martian surface samples. More recently, the European space science community has expressed general interest in the concept of cooperative Mars exploration and sample return. The USSR has now announced plans for a program of Mars exploration incorporating international cooperation. If the opportunity becomes available to participate in Mars exploration, interest is likely to emerge on the part of a number of other countries, such as Japan and Canada. The Space Studies Board's Committee on Cooperative Mars Exploration and Sample Return was asked by the National Aeronautics and Space Administration (NASA) to examine and report on the question of how Mars sample return missions might best be structured for effective implementation by NASA along with international partners. The committee examined alternatives ranging from scientific missions in which the United States would take a substantial lead, with international participation playing only an ancillary role, to missions in which international cooperation would be a basic part of the approach, with the international partners taking on comparably large mission responsibilities. On the basis of scientific strategies developed earlier by the Space Studies Board, the committee considered the scientific and technical basis of such collaboration and the most mutually beneficial arrangements for constructing successful cooperative missions, particularly with the USSR.

Levy, Eugene H.↗

NASA NTRS1997

Gas Chromatographic Detectors for Exobiology Flight Experiments

Exobiology flight experiments require highly sensitive instrumentation for in situ chemical analysis of the volatile chemical species that occur in the atmospheres and surfaces of various bodies within the solar system. The complex mixtures encountered place a heavy burden on the analytical instrumentation to detect and identify all species present. Future missions to Mars', comets, or planetary moons such as Europa, will perform experiments with complex analyses. In addition, instrumentation for such missions must perform under severely restricted conditions with limited resources. To meet these analytical requirements, improved methods and highly sensitive yet smaller instruments must continually be developed with increasingly greater capabilities. We describe here efforts to achieve this objective, for past and future missions, through the development of new or the improvement of existing sensitive, miniaturized gas chromatographic detectors.

Kojiro, Daniel R.↗

NASA NTRSDate not supplied

FORWARD AND INVERSE L-BAND RADIATIVE TRANSFER MODELING OVER THE DRY CHACO, USING SMOS OBSERVATIONS, LAND SURFACE MODELING AND IN SITU DATA

Passive microwave L-band remote sensing is well known for its sensitivity to surface soil moisture over land.The signal is also affected by other dynamic variables such as vegetation and soil salinity. In this research, L-band microwave observations of the Soil Moisture Ocean Salinity (SMOS) mission are used to explore soil surface salinity, moisture and vegetation, in the Argentinean Dry Chaco, an area with possible emerging dryland salinity. A Radiative Transfer Model (RTM) with inclusion of a correction to the soil’s dielectric constant for salinity was used in forward and inverse mode, using either in situ data or Catchment Land Surface Model (CLSM) simulations as RTM input. The forward analysis pointed out shortcomings in the modeled soil moisture and soil surface temperature estimates. The impact of salinity on forward simulations over the Dry Chaco was limited.The RTM inversion using 10 years of SMOS brightness temperature observations resulted in realistic estimates of vegetation and roughness, both with and withouto ptimizing a correction term for the dielectric constant in terms of salinity equivalents. However,the retrieval of the correction term to the dielectric constant was very uncertain and not representative of soil surface salinity, but rather of open water, texture uncertainty or soil moisture bias.

L-band↗

DOE OSTI2020

In situ liquid SIMS analysis of uranium oxide

Trace analysis of nuclear materials in solid particles collected in the environment or particles in liquid slurry generated in nuclear material manufacturing processes can pinpoint elemental, organic, and isotopic signatures of nuclear fuel cycle activities and processes. Such information can support nuclear safeguards programs by increasing our ability to detect undeclared nuclear materials, routine activities for safeguarding at declared facilities, and illicit activities. However, trace radioactive material analysis in liquids and slurries is challenging using bulk approaches. For example, one drawback of sensitive analysis such as inductively coupled plasma mass spectrometry (ICP-MS) is that sample is consumed or destroyed as a result of the technical approach. We developed a vacuum compatible microfluidic interface to enable surface analysis of liquids and liquid-solid interactions using time-of-flight secondary ion mass spectrometry (ToF-SIMS). In this work, we illustrate initial results of liquid standards containing uranium using in situ liquid SIMS. Specifically a series of diluted uranium standards used for ICPMS analysis were studied and the limit of detection was estimated. Since the liquid SIMS analysis is almost nondestructive, the same sample can be analyzed by other more destructive approaches afterwards or saved for future references. Consequently, multimodal analysis is possible. Our results demonstrate that in situ liquid SIMS can be used as a new approach to analyze radioactive materials in liquid and slurry forms of relevance to the IAEA safeguards missions.

In situ liquid ToF-SIMS, uranium, limit of detecti↗